The removal and detection of toxic analytes, including monomers and plasticizers, is important for both health and the environment. Potential absorbents and/or sensing materials are successfully made from polyaniline (PANI) and PANI doped with 10 wt.% of aluminum oxide (PANI‐Al2O3) and titanium dioxide (PANI‐TiO2). The amount of metal oxide incorporated into the surface layers of the polymer and the total amount incorporated are confirmed by energy dispersive X‐rays (EDX) and microwave plasma‐ atomic emission spectroscopy (MP‐AES), respectively. All three materials are evaluated as potential sensing materials and/or absorbents for styrene, monobutyl phthalate (MBP), and dibutyl phthalate (DBP) at 100 ppm in aqueous solutions. It is found that incorporating TiO2 into PANI improved both the sensitivity and selectivity to styrene, making PANI‐TiO2 a good absorbent and potential sensing material for styrene. Additionally, incorporating Al2O3 into PANI improved the sorption to MBP, but reduced the selectivity. As a proof‐of‐concept, the responses of the polymeric nanocomposites are combined and analyzed using principal component analysis (PCA) as such an algorithm. The output reveals good separation of the responses to each analyte, thereby demonstrating how sensing materials with poorer selectivity can be used together to overcome limitations in selectivity. Polyaniline doped with TiO2 and Al2O3 nanoparticles is evaluated for their sorption of styrene and phthalates in aqueous media. The sensing mechanisms and proof‐of‐concept demonstration of a sensing array is also included.